US 2299807 A
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' Patented Oct. 21, 1942 TREATMENT OF 'CELLULOS IC TEXTILE MATERIALS Charles lb uiibar, Blaclrley, Manchester, England.
assign ited, a co No Drawing: abpueati% 277,566. In Great 4 Claims.
This invention relates to a treatment of cellulosic textile materials, and particularly to a treatment of cellulosic textile materials whereby they are endowed with softness and with non-creasing resistant to washing. a Y It is known to treat cellulosic textile materials properties, which properties are at the same time with synthetic resins, with synthetic resin cornponents or with low molecular weight condensationproducts of synthetic resin components, the treated, materials being subsequently subjected to a process whereby there is produced a higher v degree of polymerisation of theresinous com ponents, with the object of' imparting to the cellulosic textile materials non-crushing and noncreasing properties. Such, treated cellulosic materials have a harsh feel and are stiffer than is 'pleasant or. desirable.
v This invention has as an object to devise a methodwhereby cellulosic materials can be given non-crushing and non-creasing'properties without giving them a harsh feel or unduly stiil'en- ,ing the fabric. A further object is to devise such 'a method whereby the non-crushing and nonvcreasing properties. will be resistant to washing.
A still ,lurther object-isfto provide non-creasing and non-crushing cellulosic materials whicnwill biects will appear hereinafter.- These objects reaccomplished by the following invention. I have discovered that I can achieve these objects if the textile materials are treated with an-aqueous dispersion of 'an ethyIene'p lymer ,1 T andare treated either simultaneously or before 1 or after with a medium comprising a, synthetic resin, synthetic resin components or with low molecular weight condensation products of synments being followed by drying, and by a heat treatment process at a temperature substantially greater than the softening temperature of the ethylene polymer with or without the application of mechanical pressure. a
The ethylene polymers to be used for the purposes of this invention are obtained by subjecting ethylene, with or without a small content of oxygen, to a very high pressure and a moderately elevated temperatur'eas described in United States Patent No; 2,153,553. The mention of ethylene polymers herein is intended to include in addition to the simple polymers the ethylene interpolymers and derivatives of the simple polymers,
imperial Chemical Industries Limion of Great Britain m e 5', 1939, Serial No.
ritain June 10, 1938 inotbe stiffnor have a harsh feel and which will retain these properties after washing; Further tile material itself.
.thetic resin components, the treatment or treatfor example, suchas described in British-Speciiication No. 497,643 and in Britishspecification No. 481,515. The solid simple ethylene polymers obtained as outlined above melt or soften above about C., usually between C. and 200 0., depending upon the molecular weight of the particular polymer, havehigh molecular weights ranging from 2000 upwards to 24,000 or even higher, e, g. 30,000 or 40,000, and are essentially saturated products corresponding in composition substantially to (CH2).1:. They are soluble in xylene at its boiling point and are unaffected by prolonged contact with air at ordinary temperature. These solid simple-polymers as ordinarily prepared show a crystalline structure when subiected to X-ray diffraction analysis. The molecular weights mentioned are the approximate valwas determined by the method devised by H. Staudinger (see Berichte der deutschen Chemischen Ges., 1934, 67B, 1247 et seq.). The melting. or softening. points are the values obtained by the ball and ring method. r
The aqueous dispersions of the ethylene poly mers, with which there may also be incorporated a proportion of a dispersing or emulsifying agent, such as. for example, triethanolamine stearate, are prepared, for example, by the method de scribed in the specification of British application No. 16,892/38.
The synthetic resins to be used for the process of the invention are obtained by the polymerisa-i tion of urea or thiourea or derivatives-thereof or a phenol, with an aldehyde or an aldehyde-yielding substance; there may also be used low molecular weight condensation products of these substances, or there may be ,used in tlietsube stances themselves, the said substances being subsequently condensed and polymerised on the tex- It is preferred to use the products derived from urea and formaldehyde or formaldehyde-yielding substances; particularly suitable are the low molecular weight condensation products from these substances. Suitable compositions and methods for their applications to textiles are described, for example, in British Specifications Nos. 291,474, 304,900, 431,703' and In carrying the preferred practice of the .in-'
vention into effect the cellulosic textile materials are impregnated with the aqueous dispersion of the ethylene polymer to-which has beenadded a low molecular weight condensation product of the resin compohents or to which lies been added ,proportions'otthe resin components themselves.
The treated materials are squeezedor centrifuged, dried and subjected to a heat treatment at a tem- 55 perature substantially greater than the softening point of the ethylene polymer, for example. at a temperature of 100-130 C. If desired, the textile materials may be treated in two stages, wherein the low molecular weight condensation products of the resin components or the resin com ponents themselves are applied thereto, from an aqueous medium, either before or after the application of the aqueous dispersion of the ethylene polymer. It is preferred to applythe treatin solutions to the materials in such amounts and in such concentrations, that there is deposited on the finished textile materials between 1% and of their weight of the ethylene polymer.
The invention is illustrated but not limited by the following examples in which the parts are by weight.
Example 1 A mixture of 200 parts of urea, 450 parts of neutral 40% formaldehyde and -16 parts of ammonia (sp, gr. 0.880) is boiled for 2 minutes and then cooled rapidly. To this 1. ixture is added 5'70 parts of water, 216 parts of a aqueous disper- -of 50 C. for 5 minutes in a solution containing 2 parts of soap and 5 parts of soda in 1000 parts of water, rinsed and dried. The fabric has a full soft handle and is resistant to creasing.
The aqueous dispersion of ethylene polymer used in this example was prepared as follows:
100 parts of ethylene polymer (molecular weight less than 20,000), parts of stearic acid and 12.5 parts of triethanolamine were mixed with 1000 parts of trichloroethylene and the mixture was heated at a temperature of 70-90" C.
- under a reflux condenser until the polymer was dissolved. To the hot solution -was added, with stirring, 570 parts of water containing 3.3 parts of potassium hydroxide, previously heated to a temperature of ,60-70" C. The emulsion so obtained was passed through a valve-homogeniser,
' removed therefrom, stirred and maintained at a temperature of 6080 C., whilst a stream of moist air was passed over the stirred liquid, so that the trichloroethylene was volatilised.
Example 2 A solution of a low molecular weight condensation product of urea and formaldehyde is prepared by mixing together 220 parts of urea, 440 parts of 40% formaldehyde and 18 parts of ammonia (sp. gr. 0.880), bdiling t e mixture for' 2 minutes and then cooling it rapidly. To this cold mixture is then added a solution of 15 parts of ammonium dlhydrogen phosphate, in 150 parts of water, together with suflicient water to bring the density to 20 Tw. V
Material made from yarns composed of viscose rayon staple fibre is impregnated with this solution, squeezed so that the material retains its own weight of the solution, dried at 60 C., heated at 125 C. for 4 ininutes, washed in a solution containing sodium carbonate and /4% soap at 50 C. for 5 minutes, rinsed in water, and dried.
" The so treated material is impregnated with a mixture of 1 part of the aqueous dispersion of the of ltaconic acid prepared according to the meth- I 0d of Example 5 of the specification of British application No. 16,892/38', filed June 7, 1938, and 4 parts of water, squeezed so that the material retains about its own weight of the mixture at 60 C. and heated at 125 C. for 2 minutes. The treated material has a full soft handle and is resistant to creasing.
Example 3 dispersion, dried and heated at 125 C. for 4' minutes. The material is then treated with a solution of a low molecular weight condensation product of urea and formaldehyde, dried, heated, washed, rinsed and dried as described in Example 2. The treated material has a soft handle associated with anti-crease properties.
Example 4 Spun viscose dress material is treated with a solution of a low molecular weight condensation product of urea and formaldehyde, dried, heated, washed, rinsed and dried as described in Example 2. The treated material is'then impregnated with a mixture of 1 part of theaqueous dispersion of the chlorinated ethylene polymer pre-- pared according to the method of Example 6 of the specification of British application No. 16,892/38, and 3 parts of water, squeezed so that it retains about its own weight of the mixture, dried and heated at 110 C. for 3 minutes. 'The after treatment with the chlorinated ethylene polymer dispersion confers a soft handle on the material without impairing its anti-crease properties.
As many apparently widely different embodiments of the invention may be made without departing from the spirit and scope thereof, it is to be-understoodthat the invention is not limited to the specific embodiments thereof except as defined in the appended claims.
I, claim: I
1. A process for obtaining textile materials characterized by softness and by non-creasing and non-crushing properties, said process comprising impregnating said material with an aqueous dispersion of ethylene polymer and with a substance selected from the class consisting of urea-formaldehyde and phenol-formaldehyde resins and ingredients forming such resins upon heat-treatment, and heating the textile material thus treated above the softening point of said ethylene polymer, said ethylene polymer being a solid at normal temperatures, corresponding in composition substantially to (CH-2):. and by X-ray diffraction analysis showing a crystalline structure.
2. The process set forth in claim 1 in which 4 there is deposited on the textile material between interpolymer of ethylene and the diethyl ester 1% and 5% of its weight of the ethylene polymer.
3. A process which comprises treating textile material with an aqueous dispersion of a mixture comprising ethylene polymer and a substance selected from the class consisting of urea-formaldehyde and phenol-formaldehyde resins and ingredients forming such resins upon heat-treatment, and heating the textile material thus treated above the softening point of said ethylene polymer, said ethylene polymer being a solid at normal temperatures, corresponding in composition substantially to (CH2)=, and by X-ray diffraction analysis showing a crystalline structure.
4. Textile material which is characterized by softness and by non-creasing and non-crushing properties and which is impregnated with an ethylene polymer and with a synthetic resin, said ethylene polymer being a solid at normal temperatures, corresponding in composition substantially to (CH2) 1, and by x-ray diflraction analysis showing a crystalline structure, said synthetic resin being selected from the class consisting of urea-formaldehyde and phenol-formaldehyde resins.